CN104099486A - Leaching separation method for ion-absorbed rare earth deposits - Google Patents
Leaching separation method for ion-absorbed rare earth deposits Download PDFInfo
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Abstract
The invention relates to a leaching separation method for ion-absorbed rare earth deposits. The method comprises the following steps: (1) taking ion-absorbed rare earth deposits and filling a glass column with a height of 500 mm and a diameter of 50 mm with the ion-absorbed rare earth deposits; (2) respectively preparing solutions with mass fraction of 2% from ammonium sulfate, ammonium chloride and ammonium nitrate and mixing any two of the prepared solutions according to a mass ratio of 1: 1-3 so as to prepare a composite ammonium salt leaching agent; (3) dropwise adding the leaching agent on the rare earth deposits in the glass column at a speed of 0.1 to 2 ml/min, wherein a liquid-solid ratio of the leaching agent and the rare earth deposits is 1: 1-10, carrying out continuous leaching and collecting leachate; and (4) concentrating the leachate until precipitation of a solid begins and carrying out drying at 110 DEG C so as to obtain enriched rare earth deposits. According to detection results of the enriched rare earth deposits, a leaching rate is higher than 94.5% and purity reaches more than 93.2%. The method has the advantages of low cost, simple operation, a high leaching rate, high product purity, short process time, low energy consumption and great economic benefits.
Description
Technical field
The invention belongs to a kind of method of rare-earth mineral separation and concentration, relate in particular to a kind of weathered superficial leaching rare-earth ore and drench the separation method soaking.
Background technology
China is rare earth resources storage big country, is also rare-earth products production, application and big export country simultaneously.At present, rare earth is widely used in the fields such as petrochemical complex, metallurgy, material, electronics, medical science, and rare earth is mainly derived from the extraction of ore.The ore grade of weathered superficial leaching rare-earth ore is low, ore grain size is thinner, rare earth is mainly attracted on clay mineral with hydrated ion or hydroxyl hydrated ion, adopts the conventional physical concentration such as magnetic separation, the gravity treatment method cannot enrichment rare earth, can only adopt chemical mineral processing method recovering rare earth.Taking ion as main feature, adopt electrolyte solution to carry out ion-exchange leaching rare earth according to weathered superficial leaching rare-earth ore; In recent years, in-situ lixiviation processing has solved the problems such as vegetation destruction, " removing mountain " motion and soil erosion.Such as light Yongfu (light Yongfu. research and the application [J] of In-situ leaching in rare-earth mineral. non-ferrous metal design, 2006,33 (1): 7-10.) in the situation that not destroying mining area surface vegetation, by shallow well, leaching agent solution is directly injected to ore body, leaching agent solution infiltrates ore body along the hole of rare-earth mineral, with certain flow velocity uniformly penetrating.Leaching agent solution is under gravity and ambient pressure effect, in ore hole, spread and squeeze out crevice water, positively charged ion in leaching agent solution exchanges with the rare earth ion that is adsorbed on rare-earth mineral surface simultaneously, further be diffused in solution, generate porous dehiscence gap re dip solution, then re dip solution flows into intercepting gutter, collects leaching liquid and concentrates and enrichment processing.Separately there is report (Lu Shengliang, Lu Chaohui, Wu Nanping. ion-adsorption type rare earth ore post soaks experimental study [J]. In Jiangxi Science, 1998,16 (2): 77-83.), according to the ore soaking machine reason of weathered superficial leaching rare-earth ore, adopt post soaking technology leaching rare earth, this technique can soak that performance is good, and leaching agent consumption is little, and resource utilization is high.But because the formation of weathered superficial leaching rare-earth ore bed is complicated and not deep enough and comprehensive to the research of Situ Leaching method, still exist rare earth leaching rate low, the problems such as leach liquor foreign matter content height.
Summary of the invention
Object of the present invention is just to provide that a kind of cost is low, simple to operate, leaching rate is high, and the weathered superficial leaching rare-earth ore that leach liquor foreign matter content is low drenches the separation method soaking.
A kind of weathered superficial leaching rare-earth ore of the present invention drenches the separation method soaking, and comprises the steps:
1. get weathered superficial leaching rare-earth ore, pack high 500mm into, in the glass column of diameter 50mm;
2. ammonium sulfate, ammonium chloride, ammonium nitrate are mixed with respectively to massfraction and are 2% solution, select any two kinds of solution to be mixed into ammonium salt compound leaching agent by 1: 1～3 mass ratio;
3. by above-mentioned leaching agent and rare-earth mineral by 1: 1～10 liquid-solid ratio with drip in the rare-earth mineral in glass column with the speed of 0.1～2ml/min, carry out Continuous leaching, collect leach liquor;
4. leach liquor is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral of enrichment; After testing, leaching rate is higher than 94.5% for the rare-earth mineral of this enrichment, and purity reaches more than 93.2%.
One of the preferred method of the present invention comprises the steps:
1. take weathered superficial leaching type heavy rare earths ore deposit, Longnan, 500g Jiangxi, its middle-weight rare earths grade is 1.5%; Packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium sulfate and ammonium chloride are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium sulfate and ammonium chloride and be mixed into ammonium salt compound leaching agent by the mass ratio of 1: 3;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1: 5 with the speed of 0.1～0.6ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.3g of enrichment, after testing, leaching rate is 98.6%, and the purity of rare-earth mineral is 96.6%.
Two of the preferred method of the present invention comprises the steps:
1. take weathered superficial leaching type heavy rare earths ore deposit, Longnan, 500g Jiangxi, wherein rare-earth mineral grade is 1.5%; Packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium nitrate and ammonium sulfate are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium nitrate and ammonium sulfate and be mixed into ammonium salt compound leaching agent by the mass ratio of 1:1.25;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1:1 with the speed of 1.5～2.0ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.2g of enrichment, after testing, leaching rate is 98.0%, and the purity of rare-earth mineral is 96.0%.
Described weathered superficial leaching type heavy rare earths green ore is for taking from weathered superficial leaching type heavy rare earths ore deposit, Longnan, Jiangxi.
The prepared enrichment rare-earth mineral of the inventive method, adopt the leaching rate of EDTA volumetric determination rare earth and analyze calcination and obtain the purity of rare earth oxide product by oxalic acid weighting method, concrete operation method is shown in institute of Baotou rare earth institute volume. rare earth analysis handbook [M], packet header: China rare earth association, 1995:19-137..
The present invention is from weathered superficial leaching rare-earth ore Ore Deposit Features and mineralogy, can soak characteristic by lab simulation weathered superficial leaching rare-earth ore stone original place, utilize ammonium salt compound to inject the rare earth ion generation exchange interaction Extraction of rare earth of ore body and ore body, because ammonium salt solution viscosity is little, good penetrability in rare-earth mineral, be conducive to improve drench and soak earth solution concentration, improve the leaching rate of rare earth, reduce foreign matter content in solution; Meanwhile, utilize some metal ion in rare-earth mineral to react generation precipitation with acid ion in leaching agent, be deposited in rare-earth original ore, be conducive to the leaching of rare earth ion.By optimizing leaching technology, can solve rare earth leaching rate low, the problems such as leach liquor foreign matter content height, meanwhile, have saved the process time, reduce energy consumption, have improved economic benefit.
The present invention compared with prior art, has advantages of as follows:
1. raw material sulphuric acid ammonium, ammonium chloride, ammonium nitrate etc. have easily been bought on market, and cost is lower;
2. adopt the rare earth ion generation exchange interaction Extraction of rare earth of ammonium salt compound injection ore body and ore body, simple to operate;
3. utilize ammonium salt solution viscosity little, good penetrability in rare-earth mineral, is conducive to improve drench and soaks earth solution concentration, improves the leaching rate of rare earth, reduces foreign matter content in solution; Meanwhile, utilize some metal ion in rare-earth mineral to react generation precipitation with acid ion in leaching agent, be deposited in rare-earth original ore, be conducive to the leaching of rare earth ion;
4, the present invention, by the disclosed method in light Yongfu, in the situation that not destroying mining area surface vegetation, directly injects ore body by shallow well by leaching agent solution, and leaching agent solution infiltrates ore body along the hole of rare-earth mineral, with certain flow velocity uniformly penetrating.Adopt ammonium salt compound to drench to soak the leaching rate of the rare-earth mineral that enrichment obtains behind the weathered superficial leaching type heavy rare earths ore deposit in original place, Longnan, Jiangxi more than 94.5%, rare-earth mineral (containing the rare earth oxides such as yttrium, europium, cerium) is more than purity to 93.2%, illustrate that the inventive method is feasible, and there is good leaching effect.
Embodiment
Embodiment 1
1. take 500g and take from weathered superficial leaching type heavy rare earths ore deposit, Longnan, Jiangxi, wherein rare-earth mineral grade is 1.5%, is packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium sulfate and ammonium chloride are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium sulfate and ammonium chloride and be mixed into ammonium salt compound leaching agent by 1: 3 mass ratio;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1: 5 with the speed of 0.1～0.6ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.3g of enrichment, after testing, leaching rate is 98.6%, and the purity of rare-earth mineral is 96.6%.
Embodiment 2
1. take 500g and take from weathered superficial leaching type heavy rare earths ore deposit, Longnan, Jiangxi, wherein rare-earth mineral grade is 1.5%, is packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium chloride and ammonium sulfate are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium chloride and ammonium sulfate and be mixed into ammonium salt compound leaching agent by 1: 2 mass ratio;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1: 2 with the speed of 0.6～1ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.1g of enrichment, after testing, leaching rate is 96.5%, and the purity of rare-earth mineral is 93.8%.
Embodiment 3
1. take 500g and take from weathered superficial leaching type heavy rare earths ore deposit, Longnan, Jiangxi, wherein rare-earth mineral grade is 1.5%, is packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium nitrate and ammonium chloride are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium nitrate and ammonium chloride and be mixed into ammonium salt compound leaching agent by 1: 1.67 mass ratio;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1: 8 with the speed of 1～1.5ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.2g of enrichment, after testing, leaching rate is 97.2%, and the purity of rare-earth mineral is 95.2%.
Embodiment 4
1. take 500g and take from weathered superficial leaching type heavy rare earths ore deposit, Longnan, Jiangxi, wherein rare-earth mineral grade is 1.5%, is packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium nitrate and ammonium sulfate are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium nitrate and ammonium sulfate and be mixed into ammonium salt compound leaching agent by 1: 1.25 mass ratio;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1: 1 with the speed of 1.5～2.0ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.2g of enrichment, after testing, leaching rate is 98.0%, and the purity of rare-earth mineral is 96.0%.
Embodiment 5
1. take 500g and take from weathered superficial leaching type heavy rare earths ore deposit, Longnan, Jiangxi, wherein rare-earth mineral grade is 1.5%, is packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium chloride and ammonium nitrate are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium chloride and ammonium nitrate and be mixed into ammonium salt compound leaching agent by 1: 1.56 mass ratio;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1: 1.25 with the speed of 0.9～1.3ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.0g of enrichment, after testing, leaching rate is 95.3%, and the purity of rare-earth mineral is 93.8%.
Embodiment 6
1. take 500g and take from weathered superficial leaching type heavy rare earths ore deposit, Longnan, Jiangxi, wherein rare-earth mineral is 1.5% containing grade, is packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium sulfate and ammonium nitrate are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium sulfate and ammonium nitrate and be mixed into ammonium salt compound leaching agent by 1: 1.1 mass ratio;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1:10 with the speed of 1.5～1.8ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.1g of enrichment, after testing, leaching rate is 96.5%, and the purity of rare-earth mineral is 94.1%.
Claims (4)
1. weathered superficial leaching rare-earth ore drenches the separation method soaking, and it is characterized in that comprising the steps:
1. get weathered superficial leaching rare-earth ore, pack high 500mm into, in the glass column of diameter 50mm;
2. ammonium sulfate, ammonium chloride, ammonium nitrate are mixed with respectively to massfraction and are 2% solution, select any two kinds of solution to be mixed into ammonium salt compound leaching agent by 1: 1～3 mass ratio;
3. by above-mentioned leaching agent and rare-earth mineral by 1: 1～10 liquid-solid ratio with drip in the rare-earth mineral in glass column with the speed of 0.1～2ml/min, carry out Continuous leaching, collect leach liquor;
4. leach liquor is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral of enrichment; After testing, leaching rate is higher than 94.5% for the rare-earth mineral of this enrichment, and purity reaches more than 93.2%.
2. a kind of weathered superficial leaching rare-earth ore according to claim 1 drenches the separation method soaking, and it is characterized in that comprising the steps:
1. take weathered superficial leaching type heavy rare earths ore deposit, Longnan, 500g Jiangxi, its middle-weight rare earths grade is 1.5%; Packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium sulfate and ammonium chloride are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium sulfate and ammonium chloride and be mixed into ammonium salt compound leaching agent by the mass ratio of 1: 3;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1: 5 with the speed of 0.1～0.6ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.3g of enrichment, after testing, leaching rate is 98.6%, and the purity of rare-earth mineral is 96.6%.
3. a kind of weathered superficial leaching rare-earth ore according to claim 1 drenches the separation method soaking, and it is characterized in that comprising the steps:
1. take weathered superficial leaching type heavy rare earths ore deposit, Longnan, 500g Jiangxi, wherein rare-earth mineral grade is 1.5%; Packed into high 500mm, in the glass column of diameter 50mm;
2. ammonium nitrate and ammonium sulfate are mixed with respectively to massfraction and are 2% solution, get two kinds of solution of ammonium nitrate and ammonium sulfate and be mixed into ammonium salt compound leaching agent by the mass ratio of 1: 1.25;
3. above-mentioned leaching agent and rare-earth mineral are dripped in the rare-earth mineral in glass column continuously by the liquid-solid ratio of 1: 1 with the speed of 1.5～2.0ml/min, collect leach liquor;
4. the leach liquor of collection is concentrated into and starts to have solid to separate out, then dry at 110 DEG C, obtain the rare-earth mineral 7.2g of enrichment, after testing, leaching rate is 98.0%, and the purity of rare-earth mineral is 96.0%.
4. drench according to a kind of weathered superficial leaching rare-earth ore described in claim 1 or 2 or 3 separation method soaking, it is characterized in that: described weathered superficial leaching rare-earth ore is for taking from weathered superficial leaching type heavy rare earths ore deposit, Longnan, Jiangxi.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105087925A (en) * | 2015-10-11 | 2015-11-25 | 江西理工大学 | Auxiliary leaching agent for ion-type rare earth ore leaching and ore leaching method thereof |
| CN105821207A (en) * | 2016-04-01 | 2016-08-03 | 江西理工大学 | Rare earth ore leaching agent and leaching process |
| CN106591577A (en) * | 2016-12-31 | 2017-04-26 | 武汉工程大学 | Rapid leaching method for weathered crust strain amass-type rare earth ore in which seepage is difficult |
| CN111482452A (en) * | 2020-04-03 | 2020-08-04 | 武汉工程大学 | Gradient leaching technology of weathering crust elution-deposited rare earth ore residual leaching agent |
-
2013
- 2013-04-09 CN CN201310120020.8A patent/CN104099486A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105087925A (en) * | 2015-10-11 | 2015-11-25 | 江西理工大学 | Auxiliary leaching agent for ion-type rare earth ore leaching and ore leaching method thereof |
| CN105821207A (en) * | 2016-04-01 | 2016-08-03 | 江西理工大学 | Rare earth ore leaching agent and leaching process |
| CN106591577A (en) * | 2016-12-31 | 2017-04-26 | 武汉工程大学 | Rapid leaching method for weathered crust strain amass-type rare earth ore in which seepage is difficult |
| CN106591577B (en) * | 2016-12-31 | 2019-05-03 | 武汉工程大学 | A kind of difficult infiltration weathered superficial leaching rare-earth ore Rapid Leaching method |
| CN111482452A (en) * | 2020-04-03 | 2020-08-04 | 武汉工程大学 | Gradient leaching technology of weathering crust elution-deposited rare earth ore residual leaching agent |
| CN111482452B (en) * | 2020-04-03 | 2022-05-10 | 武汉工程大学 | Gradient leaching technology of weathering crust leaching type rare earth ore residual leaching agent |
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Application publication date: 20141015 |